High Throughput Quantitative Bioanalytical LC/MS/MS Determination of Gemifloxacin in Human Urine
A highly specific, sensitive, and rapid method, to quantify gemifloxacin in human urine using HPLC coupled to the triple quadrupole mass spectrometer system, was developed and validated. Gemifloxacin and ofloxacin (internal standard) were rapidly extracted from urine samples without any tedious pret...
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| Format: | Article |
| Language: | English |
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Wiley
2013-01-01
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| Series: | Journal of Chemistry |
| Online Access: | http://dx.doi.org/10.1155/2013/905704 |
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| author | Adnan A. Kadi Rihab F. Angawi Mohamed W. Attwa Hany W. Darwish Ali Saber Abdelhameed |
| author_facet | Adnan A. Kadi Rihab F. Angawi Mohamed W. Attwa Hany W. Darwish Ali Saber Abdelhameed |
| author_sort | Adnan A. Kadi |
| collection | DOAJ |
| description | A highly specific, sensitive, and rapid method, to quantify gemifloxacin in human urine using HPLC coupled to the triple quadrupole mass spectrometer system, was developed and validated. Gemifloxacin and ofloxacin (internal standard) were rapidly extracted from urine samples without any tedious pretreatment procedure. Urine samples were filtered through a Millex-GP, 0.22 μm syringe filter. Optimal chromatographic separation of the analytes was achieved on Zorbax SB-C18 (30 mm × 2 mm i.d., 3.5 μm maintained at ambient temperature). The mobile phase consisted of 0.1% formic acid (pH 3.2) and acetonitrile (80 : 20) and a flow rate of 0.2 mL min−1 for 4 min. The analytes were monitored by electrospray ionization in positive ion multiple reaction monitoring mode. The method provided a linear response (r=0.9998) from a quantitation range of 5 ng mL−1 to at least 500 ng mL−1. The mean extraction recovery % of gemifloxacin from spiked human urine was 101.33 ± 2.58%. The reproducibility of the method was reliable with the intra- and inter-day precision of <2% and accuracy within 2%. The established method was reliably applied for the determination of gemifloxacin in volunteers’ urine samples with the mean recoveries of gemifloxacin from Factive tablets 320 mg > 97.0%. |
| format | Article |
| id | doaj-art-ed2c1746da814ac5a17048ee772ab4a6 |
| institution | Kabale University |
| issn | 2090-9063 2090-9071 |
| language | English |
| publishDate | 2013-01-01 |
| publisher | Wiley |
| record_format | Article |
| series | Journal of Chemistry |
| spelling | doaj-art-ed2c1746da814ac5a17048ee772ab4a62025-02-03T01:02:31ZengWileyJournal of Chemistry2090-90632090-90712013-01-01201310.1155/2013/905704905704High Throughput Quantitative Bioanalytical LC/MS/MS Determination of Gemifloxacin in Human UrineAdnan A. Kadi0Rihab F. Angawi1Mohamed W. Attwa2Hany W. Darwish3Ali Saber Abdelhameed4Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh 11451, Saudi ArabiaDepartment of Chemistry, College of Science, King Abdulaziz University, P.O. Box 54881, Jeddah 21589, Saudi ArabiaDepartment of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh 11451, Saudi ArabiaDepartment of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh 11451, Saudi ArabiaDepartment of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh 11451, Saudi ArabiaA highly specific, sensitive, and rapid method, to quantify gemifloxacin in human urine using HPLC coupled to the triple quadrupole mass spectrometer system, was developed and validated. Gemifloxacin and ofloxacin (internal standard) were rapidly extracted from urine samples without any tedious pretreatment procedure. Urine samples were filtered through a Millex-GP, 0.22 μm syringe filter. Optimal chromatographic separation of the analytes was achieved on Zorbax SB-C18 (30 mm × 2 mm i.d., 3.5 μm maintained at ambient temperature). The mobile phase consisted of 0.1% formic acid (pH 3.2) and acetonitrile (80 : 20) and a flow rate of 0.2 mL min−1 for 4 min. The analytes were monitored by electrospray ionization in positive ion multiple reaction monitoring mode. The method provided a linear response (r=0.9998) from a quantitation range of 5 ng mL−1 to at least 500 ng mL−1. The mean extraction recovery % of gemifloxacin from spiked human urine was 101.33 ± 2.58%. The reproducibility of the method was reliable with the intra- and inter-day precision of <2% and accuracy within 2%. The established method was reliably applied for the determination of gemifloxacin in volunteers’ urine samples with the mean recoveries of gemifloxacin from Factive tablets 320 mg > 97.0%.http://dx.doi.org/10.1155/2013/905704 |
| spellingShingle | Adnan A. Kadi Rihab F. Angawi Mohamed W. Attwa Hany W. Darwish Ali Saber Abdelhameed High Throughput Quantitative Bioanalytical LC/MS/MS Determination of Gemifloxacin in Human Urine Journal of Chemistry |
| title | High Throughput Quantitative Bioanalytical LC/MS/MS Determination of Gemifloxacin in Human Urine |
| title_full | High Throughput Quantitative Bioanalytical LC/MS/MS Determination of Gemifloxacin in Human Urine |
| title_fullStr | High Throughput Quantitative Bioanalytical LC/MS/MS Determination of Gemifloxacin in Human Urine |
| title_full_unstemmed | High Throughput Quantitative Bioanalytical LC/MS/MS Determination of Gemifloxacin in Human Urine |
| title_short | High Throughput Quantitative Bioanalytical LC/MS/MS Determination of Gemifloxacin in Human Urine |
| title_sort | high throughput quantitative bioanalytical lc ms ms determination of gemifloxacin in human urine |
| url | http://dx.doi.org/10.1155/2013/905704 |
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